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Experiments On Gramimetry and Precipitation Titration

This document describes the gravimetric method for determining nickel using dimethylglyoxime. Nickel salts are precipitated as nickel dimethylglyoximate by adding an ethanolic solution of dimethylglyoxime to an acidic nickel solution. The precipitate is filtered, washed, dried and weighed to determine the amount of nickel. The precipitate is soluble in mineral acids, hot water, and concentrated solutions of cobalt salts but insoluble in dilute ammonia solutions.

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Subhash Dhungel
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114 views4 pages

Experiments On Gramimetry and Precipitation Titration

This document describes the gravimetric method for determining nickel using dimethylglyoxime. Nickel salts are precipitated as nickel dimethylglyoximate by adding an ethanolic solution of dimethylglyoxime to an acidic nickel solution. The precipitate is filtered, washed, dried and weighed to determine the amount of nickel. The precipitate is soluble in mineral acids, hot water, and concentrated solutions of cobalt salts but insoluble in dilute ammonia solutions.

Uploaded by

Subhash Dhungel
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© © All Rights Reserved
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Gravimetric method

DETERMINATION OF NICKEL AS THE DIMETHYLGLYOXIMATE:


Discussion: Nice! i" #reci#itated $% the additio& o' a& etha&o!ic "o!(tio& o'
dimeth%!)!%o*ime+ i,e,H- DMG to a hot+ 'ai&t!% acidic "o!(tio& o' &ice! "a!t a&d the&
addi&) a "!i)ht e*ce"" o' a.(eo(" ammo&ia "o!(tio& /'ree 'rom car$o&ate0,The #reci#itate
i" 1a"hed 1ith co!d 1ater a&d the& 1ei)hted a" &ice!2 dimeth%!)%o*imate a'ter dr%i&)
at 33453-4C,
Ni
-6
6 -H-DMG Ni /HDMG0- 6 -H
6
H
OH O O
CH75C 8 N N8 C5CH7
CH7 5 C 8 N 6 -H
6
- 6 Ni
-6 Ni
CH7 5 C 8 N
CH75C8 N N8 C5CH7
OH
O O
H
The #reci#itate i" "o!($!e i& 'ree mi&era! acid"+ i& "o!(tio&" co&tai&i&) more tha& 94
#erce&t o' etha&o! $% vo!(me+ i& hot 1ater /4,:m) #er 344m!0 a&d i& co&ce&trated
ammo&ica! "o!(tio&" o' co$a!t "a!t"+ $(t i" i&"o!($!e i& di!(te ammo&ia "o!(tio&,+ i&
"o!(tio&" o' ammo&i(m "a!t" a&d i& di!(te acetic/ etha&oic 0 acid5"odi(m acetate
"o!(tio&",
Procedure: ;ei)h o(t acc(rate!% 4,7 to 4,< ) o' &ice! "a!t i&to a 944 m! $eaer 1ith a
"tirri&) rod, Di""o!ve it i& 1ater+ add 9 m! o' di!(te HC! /3:30 a&d di!(te to -44 m!, Heat
to =45>4C+ add a "!i)ht e*ce"" o' dimeth%!)!%o*ime rea)e&t+ a&d immediate!% add di!(te
ammo&ia "o!(tio& dro#1i"e+ 1ith co&"ta&t "tirri&) (&ti! #reci#itatio& tae" #!ace+ a&d
the& i& "!i)ht e*ce"" ,A!!o1 to "ta&d o& the "team $ath 'or -4574 mi&(te"+ a&d te"t the
"o!(tio& 'or com#!ete #reci#itatio& 1he& the red ##t ha" "ett!ed o(t, A!!o1 the #reci#itate
to "ta&d 'or 3 ho(r+ coo!i&) at the "ame time ,Fi!ter the co!d "o!(tio& thro()h a "i&tered
5)!a"" or #orce!ai& 'i!teri&) cr(ci$!e+ #revio("!% heated to 334 53-4C a&d 1ei)hed a'ter
coo!i&) i& a de"iccator, ;a"h the #reci#itate 1ith co!d 1ater (&ti! 'ree 'rom ch!oride /$%
te"ti&) 1ith A)NO7 to the 'i!trate0 a&d dr% it at 33453-4C 'or <9594 mi&(te", A!!o1 to
coo! i& a de"iccator a&d 1ei)h, Re#eat the dr%i&) (&ti! co&"ta&t 1ei)ht i" attai&ed a"
Ni /C<H=O- N-0-,
Yie!d:
Teacher?" Si)&at(re:
Ro!!, No:
Date:
EX@ERIMENT: TO DETERMINE THE @ERSENTAGE @ARITY OF @OTASSIAM
BROMIDE
THEORY:
Thi" e*#erime&t i" the #reci#itatio& titratio& i&vo!vi&) the #reci#itatio& reactio& $et1ee&
"i!ver &itrate a&d "odi(m ch!oride,
A)NO7 6 NaC! A) C! 6 NaNO7
-A)NO7 6 K- CrO< A)-CrO< 6 -KNO7
A "!i)ht e*ce"" o' A)NO7 "o!(tio& react" 1ith i&dicator K-CrO< a&d 'orm" a reddi"h
$ro1& co!or o' A)CrO<, ;he& @ota""i(m Bromide i" titrated a)ai&"t A)NO7 "o!(tio& the
Br
5
io& i" #reci#itated a" "i!ver $romide,
KBr 6 A)NO7 A)Br 6 K
6
6

NO7
5
Fir"t!% #rimar% ad"or$ed !a%er i" 'ormed a&d it 1i!! ho!d the "eco&dar% ad"or$ed
o##o"ite!% char)ed io& #re"e&ti&) the "o!(tio& ,A" "oo& a" the e.(iva!e&ce #oi&t i"
reached+A)
6
io&" are #re"e&t i& the e*ce"" 1hich are #rimari!% ad"or$ed a&d &itrate io&"
are "eco&dari!% ad"or$ed , D(ri&) titratio& the eo"i& i" ("ed a" i&dicator d(e to #re"e&ce
o' 1hich the co!or o' ##t, 1i!! cha&)e to the $ri)ht #i&i"h co!or at the e.(iva!e&ce #oi&t,
The 5ve io&" o' eo"i& 1hich are m(ch more "tro&)!% ad"or$ed+ tha& the &itrate io&" are
immediate!% ad"or$ed a&d 1i!! revea! it" #re"e&ce o' ##t, $% 'ormatio& o' #i&i"h
com#!e* o' "i!ver a&d a modi'ied eo"i& io&"+ are o& the "(r'ace 1ith the 'ir"t trace o' A)
6
io&",
PROCEDURE:
1. Preparation of 0.05 M NaCl solution:
4,=<99 )m o' "odi(m ch!oride 1a" tae& $%C 1ei)ht $% di''ere&ceC method, It
1a" the& tra&"'erred .(a&titative!% to a -94 m! vo!(metric '!a" a&d 1a" di""o!ved
i& deio&o"ed 1ater+ "hai&) co&ti&(o("!% 1hi!e addi&) to mae the "o!(tio&
homo)e&eo(",
Mo!arit% o' the "o!(tio&
2. Preparation of approx 0.05 M il!er nitrate solution:
-,3-- )m o' )ive& Si!ver &itrate "o!(tio& 1a" made -94m! $% addi&) deio&o"ed
1ater,
". tandardi#ation of t$e il!er nitrate solution %it$ odiu& C$loride:
34 m! o' Sodi(m Ch!oride "o!(tio& 1a" #i#etted o(t i& a co&ica! '!a", 3m! o' 9 D
@ota""i(m Chromate "o!(tio& 1a" added ,The& it 1a" titrated $% "!o1!% addi&)
"i!ver &itrate "o!(tio& 'rom $(rette, The additio& 1a" co&ti&(ed 1ith "hai&) ti!!
the co!or $ecome" 'ai&t reddi"h $ro1&, The titratio& 1a" carried o(t a&d three
co&c(rre&t readi&)" 1ere &oted,
'. Deter&ination of percenta(e purit) of *+r:
4,>79)m o' #ota""i(m $romide "o!(tio& 1a" tae& i& 344m! o' vo!(metric '!a"
a&d it 1a" di!(ted $% ("i&) deio&o"ed 1ater,
34m! o' KBr "o!(tio& 1a" #i#etted o(t i& co&ica! '!a", The& 7> m! o' deio&o"ed
1ater+ 3,9m! o' :M CH7COOH a&d 3m! o' eo"i& /i&dicator0 1a" added i&to
co&ica! '!a", It 1a" the& titrated 1ith "ta&dard "i!ver &itrate "o!(tio& 'rom $(rette,
The additio& 1a" co&ti&(ed 1ith "hai&) ti!! the co!or o' ##t 1a" #i&,
O+EER,-./ON:
.a0le1: tandardi#ation of il!er nitrate solution:
No, o' o$", Eo!,o' NaC!
/m!0
B(rette readi&)" 'or A)NO7/m!0 Co&c(rre&t readi&)
/m!0
I&itia! Fi&a! Di''ere&ce
.a0le 2: Deter&ination of %ei($t of *+r in t$e (i!en solution:
No, o' o$", Eo!,o' KBr
/m!0
B(rette readi&)" 'or A)NO7/m!0 Co&c(rre&t readi&)
/m!0
I&itia! Fi&a! Di''ere&ce
Result:
Calculation:

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